EDAX Insight 2013 Vol. 11 No. 2

June 2013
INSIDE
Volume 11 Issue 2
1/2
News
3
Tips and Tricks
4/5
Application Notes
6
Events
Training
Social Media
7
Employee
Spotlight
8
Customer News
EDS NEWS
WDS Joins the Team!
With the introduction of TEAM™ WDS, EDAX has
merged its Wavelength Dispersive Spectrometry (WDS)
product line into the highly successful TEAM™
Analysis System. The TEAM™ platform improves
ease of use and workflow, while streamlining all three
microanalysis techniques - Energy Dispersive
Spectroscopy (EDS), Electron Backscatter Diffraction
(EBSD) and WDS - into one common user interface.
Spectrometer setup, crystal selection and system
optimization were much more involved and time
consuming than with EDS analysis. With the launch of
TEAM™ WDS, EDAX has brought the automated set
up, ease of use and analytical intelligence of the
TEAM™ platform to WDS analysis, opening up the
analytical power of WDS to all analysts.
WDS has distinct advantages over EDS in both energy
resolution and detection limits. With energy resolution
around 10 eV compared to the EDS best of 121 eV,
WDS is able to resolve peak overlaps that present a
problem in EDS analysis. Additionally, with detection
limits better by an order of magnitude, WDS is able to
perform trace analysis that cannot be done with EDS.
The analytical advantages of WDS have always been
offset by the downside of WDS - historically, it has been
a much more difficult technique to optimize than EDS.
Figure 1. EDS spectrum in red and WDS spectrum in outline show
clearly that WDS offers much better energy resolution and peak
deconvolution than EDS.
2
EDS NEWS
(Continued from Page 1)
The TEAM™ Analysis System pairs TEAM™ WDS software with a
parallel beam WDS spectrometer. The EDAX spectrometer design can
be mounted on most EDS ports on a scanning electron microscope
(SEM), allowing the user greater freedom in system configuration
compared to alternative WDS systems. Additionally, the EDAX
spectrometer excels in a wide range of operating conditions from low
currents for beam sensitive materials to high currents more typical of
WDS analysis.
Figure 2. Smart Focus routine optimizes sample height by moving the stage in fine
increments until the maximum sweet spot (15.63 mm) is reached.
The launch of the TEAM™ WDS Analysis System brings all three
microanalysis techniques - EDS, EBSD and WDS - into one common,
easy to use interface and creates the industry’s most comprehensive
analytical system. The TEAM™ Analysis System provides EDAX’s
users with maximum insight in minimal time to solve their materials
characterization challenges.
The key to improving the usability of WDS is EDAX’s introduction
of Smart Focus, a fully automated focusing routine that provides
complete microscope optimization for WDS analysis. This Smart
feature optimizes the stage position relative to the WDS optic,
guaranteeing the highest intensity for each element.
By ensuring the highest quality data is collected on the first iteration,
Smart Focus brings a new level of speed and ease of use to WDS
analysis. With Smart Focus, the user is able to solve an EDS peak
overlap in three clicks of the mouse without going through the
process of focusing the optic.
TEAM™ WDS is completely integrated with TEAM™ EDS, allowing
the user to transition seamlessly between the techniques as required by
the sample. After collecting an EDS spectrum, the user can simply
highlight the area or peak of concern on the EDS results, and TEAM™
WDS will perform a spectral acquisition over that energy range,
displaying the two spectra side by side for comparison.
For samples with known overlaps or where trace analysis is
predetermined, the TEAM™ Analysis System is also able to collect
EDS and WDS simultaneously, maximizing productivity for the user
and providing a highly efficient workflow.
Figure 3. Side by side display of EDS and WDS spectra from an integrated
acquisition.
3
TIPS AND TRICKS
TEAM™ WDS Element Scan Simplifies Peak Separation and
Trace Element Detection Analyses
Element Scan
WDS optimization using the Element Scan routines allows the user
to tailor data collection specifically to a particular goal: fine peak
separation or trace element detection. The microanalysis data
required to solve each of these goals differs and, in the past, an
advanced level of knowledge was required to set up the WDS in
order to capture the relevant data. Now, using the TEAM™ WDS
software, these parameters are set automatically once the user
identifies the element and energy line of interest and clicks on the
analysis goal.
If your goal is
What you need is
TRACE ELEMENT
DETECTION
Highest intensity
PEAK SEPARATION
Best resolution
TEAM™ software provides
Element Scan with Better
Resolution setting
Element Scan with Higher
Intensity setting
EDS / WDS Comparison
A sample analysis is required of a fluorinated surface layer on an
iron part. Unfortunately, the energy of Fe L lines are very close to
the energy of the F K X-rays which produces an overlap situation,
Figure 1. The use of a high resolution X-ray spectrometer like WDS
is needed to resolve the F K and the Fe L lines.
The diffractors in WDS collect
X-rays over a range of energies.
Depending upon the diffractors
mounted in the WDS
spectrometer, small energy
ranges exist at the edges of these
ranges where two or more
potential diffractors can be used
Figure 1. Overlay of WDS spectrum in
to collect X-rays. The selection
outline over the broad EDS overlapping
process for the “best” diffractor
peaks in red.
can seem complicated, but is
usually delineated into Peak Separation and Trace Element
Detection acquisitions.
Peak Separation and Trace Element Detection
For a Peak Separation task, the diffractor that provides the best
spectral resolution is preferred; whereas, for a Trace Element
Detection task a diffractor with the highest sensitivity (intensity) is
preferred. If multiple diffractors are an option, the one with the
larger d-spacing is preferred for trace analysis while the one with the
smaller d-spacing is preferred for peak separation.
Figure 2. Element selection screen with options for Fe selected.
As seen at the bottom of the Element Selection screen shown in
Figure 2, the analyst has selected to analyze the sample for Fe and
has a choice of two diffractors (D3 and D4) for the L line, and one
(D1) for the K line. If the goal of the analysis is peak separation and
the L line is chosen, the TEAM™ WDS software will automatically
choose the D4 diffractor, which will give results with the best
resolution. If the goal is trace element detection, the D3 diffractor
will be used, giving the highest intensity.
The WDS Elemental
scans for each of
these diffractors is
shown in Figure 3
using the same
vertical scaling. The
intensity of the D3
diffractor is
significantly higher Figure 3. Comparison of the WDS analysis results
obtained using D3 (red) and D4 (outline) crystals.
than that of the D4
diffractor. This observation is not so important for the high F K peak
but is significant in identifying the much lower intensity Fe L lines.
However, the spectral resolution using this diffractor does not fully
separate the F K, Fe La1 and Fe Lb1 peaks. Use of the D4 diffractor
more clearly separates each of these peaks, especially the Fe La1
and Fe Lb1 peaks, for visual identification but at a reduced intensity.
Conclusion
As advances in microanalytical hardware technology improve
performance, precise software optimization becomes increasingly
more important. The Element Scan routines within the TEAM™
WDS software guarantee the best data collection possible, allowing
all users to achieve the highest level of insight into their material.
4
EDS PRODUCT NEWS
TEAM™ Trident Helps Engineer Better Wear Materials
Tungsten Carbide (WC) is a ceramic material used in many industrial
applications and is well known for its abrasion resistance and ability
to withstand high temperatures. One standard application is for cutting
tools, where the WC is typically cemented together with a binder
material, usually metal such as Cobalt (Co). The metal forms a ductile
matrix phase which counters the brittle nature of the WC grains,
raising the toughness and durability of the tool.
Table 1 shows some examples of application requirements correlated
to microstructure trait and characterization method. In each case,
advanced characterization of the cemented carbide is required to
design and control the production of the cutting tool for optimized
results. To fully understand the microstructure and the resulting
properties, engineers rely on chemical (Energy Dispersive
Spectroscopy (EDS) and Wavelength Dispersive Spectrometry
(WDS)) and structural (Electron Backscatter Diffraction (EBSD))
analysis.
Application Requirement Chemical/Structural Need Characterization Tool
High Abrasion Resistance
Small WC Grains
EBSD
Higher Binder content;
Thermal Shock Resistance characterization of the
WDS
binder and additives
High Compression
Co and C Content &
EDS/Phase Mapping
Resistance
Distribution
Table 1. WC application requirements correlated to microstructure trait and
characterization method.
High Abrasion Resistance - Grain Size Analysis (EBSD)
EBSD is an ideal characterization tool for measuring the grain size of
crystalline materials, particularly when the WC grain size approaches
the resolution limits of optical microscopy. By indexing the
orientation of grains on the sample surface, engineers are able to
measure not only grain orientation but also size, shape and distribution
and to determine materials phases.
Figure 1a. EBSD grain map showing grain structures in a WC
material where individual grains highlight size and morphology.
Grain Size (diameter)
Number Fraction
Engineers can control the properties of the cutting tool by varying the
WC grain size and the binder content in the matrix, enabling them to
maximize tool performance and lifetime for specific application needs.
For example, smaller WC grains produce a harder final product,
increasing wear resistance and decreasing erosion, but also decreasing
strength and toughness. By contrast, if the product is to operate in
thermal extremes, engineers will design tools with larger WC grains
for increased resistance to thermal shock. In terms of the binder
material, higher levels of Co will lead to an increase in crack
resistance, but decrease abrasive wear resistance.
Grain Size (Diameter) [microns]
Figure 1b. Corresponding grain size distribution resulting from
the map in figure 1a.
Figure 1a is an EBSD grain map showing grain structures in a WC
material where individual grains are randomly colored to highlight
size and morphology. Figure 1b is the corresponding grain size
distribution resulting from the map in Figure 1a. The average grain
size in this case is 880 nm.
High Compression Resistance – Co and C distribution
(EDS/Phase Mapping)
For tools operating in a high compression application, lifetime is
strongly affected by the amount of Co and C in the matrix and by the
distribution of these elements.
5
EDS PRODUCT NEWS
(Continued from Page 4)
Figure 2a. Elemental map of W (green), Co (blue) and
C (red).
Figure 2b. Standard C elemental map.
EDS elemental mapping is sufficient to examine the distribution of Co
in the microstructure, as shown in figure 2a, but C is much more
difficult because of its association with W in WC and its existence as
elemental C (see Figure 2b). Standard elemental mapping cannot
distinguish between C in different phases. EDAX’s Smart Phase
Mapping has the unique ability to be able to look at C distribution as
it relates to each phase; whereas, competitive systems provide only
overall distribution. Engineers gain invaluable insight from this
accurate depiction of the microstructure.
Conclusion
Figure 2c. Map of C from WC phase only.
EDAX’s TEAM™ Trident combines the power of EDS, EBSD and
WDS into a smart, easy to use platform and creates the most
comprehensive analysis system on the market. With complete
integration and optimum workflow, TEAM™ Trident is the ultimate
tool to solve the most difficult characterization problems, and allows
engineers to design a better tool.
Thermal Shock Resistance – Binder concentration and additives
(WDS)
The thermal shock properties of WC tools are controlled by the
varying percentage of the binder phase and with specific binder
additives to modify transport properties of the final composition.
While EDS is often sufficient to analyze the amount of binder present,
the additives are often present in minute amounts, requiring the trace
analysis capabilities of WDS. Figure 3 shows two WDS spectra from
a binder phase, one with trace Fe additive and one without. The
increased sensitivity of WDS, paired with the resolution necessary to
resolve crowded low energy X-ray lines, allows engineers to make
very small changes to binder composition and design the thermal
properties of the tool to match the application.
Figure 3. WDS spectra from two different regions of the binder phase.
6
Worldwide Events
July 7-11
Integrated Computational Materials Engineering
August 4-8
Microscopy & Microanalysis 2013
August 11-16
International Materials Research Congress
August 25-30
MC Regensburg
EVENTS AND TRAINING
September 3-6
EMAG 2013
September 18-20
Materialographie
October 27-31
MS&T 2013
November 5-6
ISTFA
Salt Lake City, UT
Indianapolis, IN
Cancun, Mexico
Regensburg, Germany
Please visit www.edax.com for a complete list of our tradeshows.
York, UK
Friedrichshafen, Germany
Montreal, Quebec, Canada
San Jose, CA
2013 Worldwide Training
To help our present and potential customers obtain the most from their equipment and to increase their expertise in EDS microanalysis, WDS
microanalysis, EBSD/OIM™, and Micro-XRF systems, we organize a number of Operator Courses at the EDAX facilities in North America;
Tilburg, NL; Wiesbaden, Germany; Japan, and China.
EUROPE
EDS Microanalysis
September 12-13, 2013
November 7-8, 2013
Tilburg
Tilburg
TEAM™ EDS
September 24-26, 2013 Tilburg
November 11-13, 2013
Wiesbaden
Genesis
November 19-21, 2013
Tilburg
EBSD
September 9-11, 2013
November 4-6, 2013
November 13-15, 2013
Tilburg
Tilburg
Wiesbaden
November 11-15, 2013
Wiesbaden
October 8-9, 2013
Tilburg
October 29-30, 2013
Wiesbaden
TEAM™ EDS & EBSD (Pegasus)
WDS LEXS
JAPAN
EDS Microanalysis
Genesis
October 10-11, 2013
Tokyo
November 14-15, 2013 Osaka
July 11-12, 2013
TEAM™ EDS
Osaka
CHINA
EDS Microanalysis
NORTH AMERICA
EDS Microanalysis
TEAM™ EDS
July 16-18, 2013
Draper, UT
September 17-19, 2013 Mahwah, NJ
EBSD OIM™ Academy
November 12-14, 2013
Mahwah, NJ
October 1-3, 2013
Mahwah, NJ
Micro-XRF
TEAM™ EDS
September 24-26, 2013 Shanghai
October 10, 2013
Xi’an
December 3-5, 2013
Shanghai
EBSD OIM™ Academy
October 15-17, 2013
Shanghai
Orbis: Course & Workshop
Presented in English
Please visit www.edax.com/support/training/index.aspx for a complete list and additional
information on our training courses.
Visit edax.com for the latest news and up-to-date product information.
7
EMPLOYEE SPOTLIGHT
Tobias Lorenz
Kim Meyer
for Germany, Austria and Switzerland. He is located in the south
as a Purchasing Clerk. She has been with EDAX in the Mahwah,
Tobias joined EDAX in November 2007 as Field Service Engineer
of Germany near Stuttgart.
Prior to EDAX, Tobias worked as a Field Service Engineer for the
Holzmann Service Group servicing domestic appliances for the
Kim joined EDAX in February 1986 in the purchasing department
NJ facility for over 27 years. Today, as a Senior Planner/Buyer,
Kim is responsible for the planning and purchasing of materials
for the manufacturing floor to meet customers’ delivery
United States Army in southern Germany from 1998-2002. In this
requirements. She works closely with the engineering department
worked as a Sales and Service Engineer for an Italian company,
suppliers and building partnerships that will benefit both EDAX
job, he improved his knowledge of the English language and
learned a lot about American culture. From 2001-2007, Tobias
Etipack Labeling Systems in Germany. Previously, he attended
vocational school where he trained as an electromechanical
technician.
Tobias and his partner, Tatjana, have lived in Waiblingen near
Stuttgart for the past three years. In his spare time, Tobias enjoys
hiking and spending time with his family, friends and dog, Vito.
on various team projects and supports the service department when
parts are needed for customers.
Kim enjoys working with
and the supplier. She is also an ISO Internal Auditor for the EDAX
organization.
Kim attended the County College of Morris where she earned an
associate’s degree in Psychology. She then went onto Montclair
State University and also attended Dutchess BOCES for additional
training in electronics.
Kim currently lives in Wappingers Falls, NY with her husband
Keith and her two children, Deanna (21) and Brandon (16).
Outside of EDAX, she has been involved with her local school
district as PTA Council President and was a parent representative
on several school committees. In her spare time, Kim enjoys
playing tennis, running/walking, reading biographies and attending
her kids’ various sports activities. She loves the hot weather and
usually heads to the beach every summer for vacation.
8
CUSTOMER NEWS
Freudenberg-NOK Sealing Technologies
Plymouth, Michigan
Freudenberg-NOK Sealing Technologies is a leading producer of
advanced sealing technologies and rubber products for a variety of
performance applications, including: aerospace, agriculture, appliance,
automotive, construction, diesel engine, energy, food and beverage,
heavy industry and pharmaceuticals. Founded in 1989, Freudenberg-
NOK is headquartered in Plymouth, Michigan with 22 facilities
throughout North America. The company also performs product
analysis and reverse engineering on samples sent from the United States,
Canada, Mexico and South America.
One of the challenges currently facing Freudenberg-NOK is detecting
silane-based adhesives on a matrix of rubber filled with silicon-based
minerals. The details of this complex process are important because
much of the company’s work deals with adhesion analysis.
To help solve this issue, Freudenberg-NOK purchased an EDAX Octane
Silicon Drift Detector (SDD).
One of the company’s busiest
instruments, the Octane SDD, along with the TEAM™ EDS Analysis
System, allows the lab chemists to quickly and effectively analyze
materials. They use the data to complement information obtained from
the company’s Fourier Transform Infrared Spectrometers, which
provide information concerning chemical structure.
“EDAX is the analysis system we are most familiar with,” stated Fred
Fraser, Analytical Lab Manager. “We have had good experiences with
the company and the equipment works very well. One other important
consideration is the organization’s ability to address technical questions.
EDAX has done this in a prompt and professional manner.”
Chemist Ryan Fleming uses an EDAX Octane Silicon Drift Detector in
Freudenberg-NOK Sealing Technologies’ Analytical Laboratory.
EDAX Inc.
91 McKee Drive
Mahwah, NJ 07430
Phone (201) 529-4880
E-mail: [email protected]
www.edax.com
Art and Layout
Jonathan McMenamin
Contributing Writers
Sue Arnell
Patrick Camus
Mike Coy
Tara Nylese
®2013 EDAX, Inc. All rights reserved.
No part of this publication may be
reproduced, stored in a retrieval
system, or transmitted in any form
or by any means without prior
written permission of EDAX Inc.